#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/48/2004808.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2004808 loop_ _publ_author_name 'Gunasekaran, K.' 'Govindasamy, L.' 'Shanmuga Sundara Raj, S.' 'Velmurugan, D.' 'Karunakaran, S.' 'Kandaswamy, M.' _publ_section_title ; 2,2'-Piperazin-1,4-diyldimethylenebis[6-(benzyliminomethyl)-4-methylphenol] ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1027 _journal_page_last 1028 _journal_volume 52 _journal_year 1996 _chemical_formula_sum 'C36 H40 N4 O2' _chemical_formula_weight 560.7 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source 'SHELX76 (Sheldrick, 1976)' _cell_angle_alpha 90 _cell_angle_beta 98.68(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.931(2) _cell_length_b 20.811(3) _cell_length_c 12.479(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 23 _cell_measurement_theta_min 15 _cell_volume 1522.6(6) _computing_data_reduction 'SDP (Frenz, 1978)' _computing_molecular_graphics 'PLUTO (Motherwell and Clegg, 1978)' _computing_publication_material 'PARST (Nardelli, 1983)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3288 _diffrn_reflns_theta_max 70 _diffrn_standards_decay_% <1.2 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_type empirical _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.223 _exptl_crystal_description needle _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.3584 _refine_diff_density_min -0.2117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.15 _refine_ls_hydrogen_treatment ;refall except the phenolic H atom which could not be located from the difference Fourier ; _refine_ls_number_parameters 266 _refine_ls_number_reflns 1698 _refine_ls_R_factor_obs 0.05 _refine_ls_shift/esd_max 0.004 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ' 1/[\s^2^(F)+0.0038F^2^]' _refine_ls_wR_factor_obs 0.06 _reflns_number_observed 1698 _reflns_number_total 2892 _reflns_observed_criterion I>=3\s(I) _[local]_cod_data_source_file pt1018.cif _[local]_cod_data_source_block pt1018a _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 1522.64 _cod_database_code 2004808 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv C1 0.5983(5) 0.1854(1) -0.18580(2) 3.85(7) C2 0.5001(5) 0.2018(1) -0.29210(2) 4.09(8) C3 0.6013(5) 0.1813(1) -0.37940(2) 4.43(6) C4 0.7969(5) 0.1448(1) -0.36560(2) 4.28(6) C5 0.8893(5) 0.1289(1) -0.25950(2) 4.03(7) C6 0.7950(5) 0.1476(1) -0.17010(2) 3.73(7) O7 0.5074(4) 0.2071(1) -0.09930(1) 5.14(5) C8 0.9113(7) 0.1237(2) -0.45970(1) 5.84(11) C9 0.2943(5) 0.2419(1) -0.31250(1) 4.78(9) N10 0.2024(4) 0.2657(1) -0.23610(2) 5.15(9) C11 -0.0086(5) 0.3034(1) -0.26520(3) 6.08(11) C12 0.0175(5) 0.3713(1) -0.22590(2) 4.04(8) C13 -0.1383(6) 0.3994(1) -0.16770(3) 5.77(11) C14 -0.1195(7) 0.4631(2) -0.13770(3) 7.01(12) C15 0.0552(8) 0.4994(2) -0.16410(3) 6.80(11) C16 0.2120(6) 0.4726(1) -0.22010(3) 5.47(9) C17 0.1920(5) 0.4093(1) -0.25060(2) 4.27(8) C18 0.9120(5) 0.1292(1) -0.05750(2) 4.32(7) N19 0.9788(3) 0.0619(1) -0.05140(1) 3.35(5) C20 0.7810(4) 0.0209(1) -0.04710(2) 3.66(5) C21 1.1511(4) 0.0492(1) 0.04270(2) 3.54(4) H3 0.537(5) 0.194(1) -0.453(2) .064(9) H5 1.024(6) 0.104(2) -0.249(3) .073(11) H81 0.852(9) 0.142(2) -0.526(4) .119(7) H82 0.903(8) 0.077(2) -0.468(4) .110(14) H83 1.049(10) 0.141(2) -0.460(4) .128(18) H9 0.231(7) 0.250(2) -0.399(3) .079(11) H111 -0.067(7) 0.304(2) -0.352(3) .106(13) H112 -0.116(7) 0.280(2) -0.233(3) .116(13) H13 -0.246(7) 0.373(2) -0.149(3) .096(12) H14 -0.227(9) 0.485(2) -0.101(4) .125(15) H15 0.066(7) 0.547(2) -0.151(3) .110(13) H16 0.333(6) 0.499(2) -0.238(3) .088(11) H17 0.298(6) 0.390(2) -0.294(3) .090(11) H181 0.800(6) 0.140(2) -0.001(3) .073(10) H182 1.036(6) 0.156(2) -0.039(3) .066(10) H201 0.682(5) 0.007(1) -0.117(2) .131(8) H202 0.727(5) 0.010(1) 0.026(2) .107(9) H211 1.098(5) 0.063(1) 0.113(2) .052(8) H212 1.286(5) 0.079(1) 0.038(2) .066(8) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C6 C1 O7 120.1(2) yes C2 C1 O7 120.8(2) yes C2 C1 C6 119.1(2) yes C1 C2 C9 121.1(2) yes C1 C2 C3 119.9(2) yes C3 C2 C9 119.0(2) yes C2 C3 C4 121.9(2) yes C3 C4 C8 122.3(2) yes C3 C4 C5 117.0(2) yes C5 C4 C8 120.8(3) yes C4 C5 C6 123.6(2) yes C1 C6 C5 118.5(2) yes C5 C6 C18 119.7(2) yes C1 C6 C18 121.7(2) yes C2 C9 N10 122.1(2) yes C9 N10 C11 117.9(3) yes N10 C11 C12 112.3(2) yes C11 C12 C17 120.9(2) yes C11 C12 C13 121.7(3) yes C13 C12 C17 117.4(3) yes C12 C13 C14 121.0(3) yes C13 C14 C15 120.1(4) yes C14 C15 C16 120.0(4) yes C15 C16 C17 120.0(3) yes C12 C17 C16 121.6(3) yes C6 C18 N19 111.9(2) yes C18 N19 C21 111.6(2) yes C18 N19 C20 110.6(2) yes C20 N19 C21 109.5(2) yes C2 C3 H3 120(2) no C4 C3 H3 118(2) no C4 C5 H5 118(2) no C6 C5 H5 119(2) no C4 C8 H83 114(3) no C4 C8 H82 111(3) no C4 C8 H81 115(3) no H82 C8 H83 116(4) no H81 C8 H83 93(4) no H81 C8 H82 108(4) no C2 C9 H9 114(2) no N10 C9 H9 124(2) no N10 C11 H112 103(2) no N10 C11 H111 112(2) no H111 C11 H112 107(3) no C12 C11 H112 113(2) no C12 C11 H111 109(2) no C12 C13 H13 116(3) no C14 C13 H13 123(3) no C13 C14 H14 124(3) no C15 C14 H14 116(3) no C14 C15 H15 123(2) no C16 C15 H15 117(2) no C15 C16 H16 117(3) no C17 C16 H16 123(2) no C16 C17 H17 121(2) no C12 C17 H17 117(2) no C6 C18 H182 108(2) no C6 C18 H181 109(2) no H181 C18 H182 105(3) no N19 C18 H182 112(2) no N19 C18 H181 111(2) no N19 C20 H202 121(2) no N19 C20 H201 119.0(10) no H201 C20 H202 119.0(10) no N19 C21 H212 108.0(10) no N19 C21 H211 112(2) no H211 C21 H212 103(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.408(3) yes C1 C6 1.399(4) yes C1 O7 1.355(4) yes C2 C3 1.388(4) yes C2 C9 1.469(4) yes C3 C4 1.376(4) yes C4 C5 1.394(3) yes C4 C8 1.508(4) yes C5 C6 1.376(4) yes C6 C18 1.518(3) yes C9 N10 1.268(4) yes N10 C11 1.475(4) yes C11 C12 1.496(3) yes C12 C13 1.388(5) yes C12 C17 1.378(4) yes C13 C14 1.377(6) yes C14 C15 1.362(6) yes C15 C16 1.364(6) yes C16 C17 1.371(3) yes C18 N19 1.454(3) yes N19 C20 1.458(3) yes N19 C21 1.460(3) yes C3 H3 0.98(2) no C5 H5 0.94(4) no C8 H81 0.93(5) no C8 H82 0.98(4) no C8 H83 0.89(6) no C9 H9 1.10(4) no C11 H111 1.09(4) no C11 H112 0.94(4) no C13 H13 0.90(4) no C14 H14 0.96(5) no C15 H15 1.00(4) no C16 H16 0.91(4) no C17 H17 0.97(4) no C18 H181 1.08(4) no C18 H182 0.92(4) no C20 H201 1.01(2) no C20 H202 1.04(3) no C21 H211 1.02(3) no C21 H212 1.02(3) no _journal_paper_doi 10.1107/S0108270195010420